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    盐析辅助分散液液微萃取结合气相色谱-质谱法测定饮料中9种常用添加剂的含量

    Determination of 9 Commonly Used Additives in Beverages by Gas Chromatography-Mass Spectrometry with Salting-Assisted Dispersive Liquid-Liquid Microextraction

    • 摘要: 为实现饮料中常用防腐剂和抗氧化剂的同时检测,进行了题示研究。取饮料样品5.000 g,加入1.0 mL 50%(体积分数)盐酸溶液和1.0 g氯化钠,超声溶解后快速注入含900 μL三氯甲烷(萃取剂)和900 μL乙醇(分散剂)的混合萃取剂,涡旋3 min,离心2 min,收集底部三氯甲烷相。再加入900 μL三氯甲烷重复萃取一次,合并两次三氯甲烷相,于40 ℃氮吹至干。加入1.0 mL乙酸乙酯复溶,过0.22 μm尼龙滤膜,滤液采用气相色谱-质谱法分析。6种防腐剂(山梨酸、苯甲酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)和3种抗氧化剂(丁基羟基茴香醚、2,6-二叔丁基对甲酚、特丁基对苯二酚)在HP5-MS UI毛细管色谱柱上以程序升温条件分离,电子轰击离子源电离,选择离子监测模式检测,外标法定量。结果显示:9种添加剂的质量浓度均在1.0~100 mg·L-1内与对应的定量离子的峰面积呈线性关系,检出限(3S/N)为0.07~0.22 mg·kg-1;以空白碳酸饮料、茶饮料和果汁饮料样品为基质进行3个浓度水平的加标回收试验,回收率为85.5%~105%,测定值的相对标准偏差(n=6)为1.2%~7.1%。方法用于22份实际样品的分析,在6份样品中检出了苯甲酸,在5份样品中检出了山梨酸,检出量均未超过GB 2760—2024规定的最大限量,且与标准方法GB 5009.28—2016的基本一致。

       

      Abstract: This study mentioned by the title was conducted to achieve simultaneous detection of commonly used preservatives and antioxidants in beverages. The 5.000 g of beverage sample was taken and mixed with 1.0 mL of 50% (volume fraction) hydrochloric acid solution and 1.0 g of sodium chloride, followed by ultrasonic dissolution. A mixed extractant containing 900 μL of chloroform (extractant) and 900 μL of ethanol (dispersant) was rapidly injected, and the solution obtained was vortexed for 3 min, and centrifuged for 2 min to collect the chloroform phase at the bottom. An additional 900 μL of chloroform was added for repeated extraction, and the two chloroform phases were combined and blown to dryness at 40 ℃ by nitrogen. The residue was reconstituted with 1.0 mL of ethyl acetate, and the solution obtained was passed through a 0.22 μm nylon filter membrane. The filtrate was analyzed by gas chromatography-mass spectrometry. The 6 preservatives (sorbic acid, benzoic acid, methylparaben, ethylparaben, propylparaben, and butylparaben) and 3 antioxidants (butylated hydroxyanisole, butylated hydroxytoluene, and tert-butylhydroquinone) were separated on HP5-MS UI capillary column using temperature programmed condition, ionized by electron impact ion source, detected in selected ion monitoring mode, and qualified by external standard method. It was shown that linear relationships between the mass concentrations of the 9 additives and peak areas of their corresponding quantitative ions were kept in the range of 1.0-100 mg·L-1, with detection limits (3S/N) in the range of 0.07-0.22 mg·kg-1. The spike recovery tests at three concentration levels were conducted using blank samples of carbonated beverage, tea beverage, and fruit juice beverage as matrices, giving recoveries in the range of 85.5%-105%, and RSDs (n=6) of the determined values in the range of 1.2%-7.1%. The proposed method was applied to the analysis of 22 actual samples, and benzoic acid in 6 samples and sorbic acid in 5 samples were detected. The detected amounts did not exceed the maximum limits specified in GB 2760—2024 and were consistent with those given by the standard method GB 5009.28—2016.

       

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